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Low-cost high-crystallinity black phosphorus and preparation method thereof

A high-crystallinity, low-cost technology, applied in the preparation of phosphorus, etc., can solve the problems of uneven black phosphorus purity, long black phosphorus cycle, and many influencing factors, and achieve low raw material prices, low production costs, and production processes. simple effect

Pending Publication Date: 2020-08-04
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of black phosphorus by red phosphorus mineralization has a long cycle, cumbersome process, many influencing factors, and high requirements for equipment.
Moreover, the reactor is a disposable consumable, and the cost is high. In addition, the purity of the black phosphorus produced varies due to the amount of catalyst.

Method used

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  • Low-cost high-crystallinity black phosphorus and preparation method thereof
  • Low-cost high-crystallinity black phosphorus and preparation method thereof
  • Low-cost high-crystallinity black phosphorus and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A low-cost high-crystallinity black phosphorus, its composition is shown in the following table:

[0035]

[0036] The steps that preparation method comprises are as follows:

[0037] (1) Mix the two-phase components according to the distribution ratio of the components and disperse evenly by magnetic stirring, the stirring speed is 600rpm, and the stirring time is 1h to obtain a red-black dispersion;

[0038] (2) According to the ratio of 30ml dispersion liquid: 50ml polytetrafluoroethylene lining, take the above dispersion liquid and add it to the polytetrafluoroethylene lining of the reactor;

[0039] (3) Tighten the polytetrafluoroethylene lining and place it in a high-temperature oven, and adjust the temperature to 180°C for 12 hours;

[0040] (4) After the reaction, the sample was washed with benzene, ethanol and water until neutral, and dried at 60° C. for 12 hours to obtain low-cost and high-crystallinity black phosphorus with a lamellar structure.

Embodiment 2

[0042] A low-cost high-crystallinity black phosphorus system, its components are shown in the following table:

[0043]

[0044] The preparation method of described low-cost high-crystallinity black phosphorus, the steps that it comprises are as follows:

[0045] (1) Mix the two phases of red phosphorus and pentamethylenediamine according to the distribution ratio of the components and disperse them uniformly by ultrasonic, the ultrasonic power is 500w, and the ultrasonic time is 1h, to obtain a red-black dispersion;

[0046] (2) According to the ratio of 30ml dispersion liquid: 50ml polytetrafluoroethylene lining, take the above dispersion liquid and add it to the polytetrafluoroethylene lining of the reactor;

[0047] (3) Tighten the polytetrafluoroethylene lining and place it in a high-temperature oven to raise the temperature to 240°C for 12 hours;

[0048] (4) After the reaction, the sample was washed with benzene, ethanol, and water until neutral, and dried at 60° C....

Embodiment 3

[0050] A low-cost high-crystallinity black phosphorus, its composition is shown in the following table:

[0051]

[0052] The preparation method of described low-cost high-crystallinity black phosphorus, the steps that it comprises are as follows:

[0053] (1) Mix the two phases of yellow phosphorus, phosphorus pentoxide and ethylenediamine according to the component distribution ratio and mechanically stir to disperse evenly, the stirring speed is 350rpm, and the stirring time is 2h to obtain a red-black dispersion;

[0054] (2) According to the ratio of 32ml dispersion liquid: 51ml polytetrafluoroethylene lining, take the above dispersion liquid into the polytetrafluoroethylene lining;

[0055] (3) Tighten the polytetrafluoroethylene lining and place it in a high-temperature oven to raise the temperature to 220°C for 12 hours;

[0056] (4) After the reaction, the sample was washed with benzene, ethanol, and water until neutral, and dried at 55°C for 13 hours to obtain la...

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Abstract

The invention discloses low-cost high-crystallinity black phosphorus which is prepared from a phosphorus source and an amine solvent through a solvothermal method, and further discloses a preparationmethod of the low-cost high-crystallinity black phosphorus. The preparation method of the black phosphorus is mild in reaction, easy to control and simple in process, and the prepared black phosphorushas very high crystallinity and oxidation resistance, can replace black phosphorus prepared by a high-temperature mineralization method in some application aspects, and can meet the requirements of people on black phosphorus performance.

Description

technical field [0001] The invention relates to the field of black phosphorus preparation, in particular to a low-cost and high-crystallinity black phosphorus and a preparation method thereof. Background technique [0002] Black phosphorus is a layered structure crystal with pleats, which is formed by transforming white phosphorus at high pressure and high temperature. Black phosphorus has the weakest reactivity among phosphorus allotropes, and it will not spontaneously ignite in air. Black phosphorus has many excellent properties: such as high specific surface area of ​​nano black phosphorus, adjustable direct band gap, good photoelectric performance and good anisotropy, etc. Based on these good properties, it has good application prospects in energy storage, optoelectronics, catalysis and other fields. The preparation of black phosphorus is relatively difficult. Most of the red phosphorus is converted into black phosphorus by high-energy ball milling. However, because th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/02
CPCC01B25/02
Inventor 谢德龙朵云霞徐杜兵谢于辉梅毅
Owner KUNMING UNIV OF SCI & TECH
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